Process of manufacturing ammonia.



FREDERICK W. FRERIGHS, OIT-ST.- LOUIS, MISSOURI.

rnocnss on MANUFACTURING AMMONIA.

specification f Letter ramena Patented Dec. A1, 190s.

Appunti@ and mm s, 1907. smal No. ascuas.

To all whom 'it maycon/cem:

Be-it known that`I,fFnEDamo1r W. Funn- Icris, a citizen of-'the UnitedStates, residing at St. Louis, in the county of St. Louis and State ofAMissouri, have invented' certain new' and useful Improvements inProcesses of Manufacturincr Ammonia; and I do hereby declare thefollowin to be a full, clear, and exact description o the invention,such as will enable others skilled in the art to which it apprtainstomake and use the same.

This invention relate's to improvements in the process of manufacturingammonia and is directed more particularly to the production ofpureannnonia from crude ammoniacal liquors.

One of theobjects of the present improved process is to obtain ammoniain a purer state and with less expense than is possible by processes nowin general use.

Another object of the resent process is to obtain commercial sul ate ofammonium freed from volatile carbon and nitrogenousorgpnic compounds.

.lhes'e objects are attained to such anextent that volatile carboncompounds and nitrogenous-organiccompounds which re main in the ammoniaand the commercial sulfate of ammonium obtained by the usual processesare removed, and the cheapness with which the present improved processmay be carried out Will/readily be appreciated by those skilled ini thcart', since only such amount of lime is required as is necessary todecompose the non-volatlle ammonia compounds contained in the ammoniacalliquor, and theoretically,.no sulfuric acid is lost in carr ing ont theprocess, only such vsulfuric aci being actually lost as escapes inhandling and by oxidation, the same sulfuric acid being used over andover.

As a conventional means for carrying into effect the present invention ndrawing is herewith presented wherein j' Figure 1 is a longitudinal,velltical, sectional view of the apparatus, and Fig. 2 a transverse,verticahsectional vie. l 4taken on line 242 of Ifig.' 1 lookingin theirection of the arrow. al

. 'l The apparatus here conventionally shown comprises a cylindrical orsubstantially c vlindrical retort within which u shaft l1 is journaledthrough the usual and ordinary packing box' or gland lQ'ahd operated by.a valve 21 1s employedV 'any approved means as the gear '13. TheVshaft. 11 carries a plurality of agitators of any approved form shownas at 14 and pipes l5 are provided through which air may be forced.

For charging the retort an openingl is provided having any'form ofclosure, and a discharge o ening 17 with a closure -is 'also provided.referably a pocket 18 4is formed 1n one end of the retort inA which athermometer 19. may rest and a pitpe 2l) controlled by or dischargingthe products of'decomposition. A pipe 22 controlled by a valve 23 isalso employed from which the ammonia gas may be discharged. The wholeretort 1s preferably set in 4the furnace presented conventionally at 24heated in any approvedmanner.

In carrying out the present improved process, the process is started byheating commercial sulfate of ammonium in a suitable still Whichfispreferably provided with an a 'tating device to a temperature sufficienty high to volatilize the carbon compounds contained in thesalt and toconvert the nitrogenous-organc compounds into sulfate of ammonium byreacting with the sulfuric acid of the ammonium salt, but care must betaken that in this period of the process the temperature is kept belowthe degree at which considerable quantities of ammonia gasare liberated-from the salt. In doing this the salt may safely be heated to 200 C.,and in order to facilitate the process of purification an air blast mabe intro duce'din the still in some suitab e' manner. lVhen all of thenitrogenous organic compounds and all of the carboncompounds which termincludes methyl alcohol, ethyl alcohol, isopropyl alcohol, acetone,benzol, toluol` naphthalin and similar compounds have been volatilizedor destroyed and the products of decomposition hare been elimi nnted,the temperature is increased to such a degree that all of the salt or amaterial proportion thereof decolnposes according to the followingformula- This takes place at or about 350 C., but the process can behastened Without destroying any ammonia by raising the temperature to400 C., in which case part of the acid sulfate ofammonium is decomposedinto pyrosulfato of amu'ioniiun and water, :wcording If the temperatureis much higher than 400" C. considerable quantitiesl ol' nitringwn areevolved which proves a dcconil'ureition and confszcqucnt lossoi ammonia.The rcs-uiting pure ammonia gas may thon ho worked into such products asmay he desired. and the acid sulfate of amnn'mimn and pyrosuliatc ofammonium 4rcsnllint r from the opi-ration are dissolved in water, andthe resulting solution of acid sulfate of ammonium is util ized forabsorbing volatile ammonium compounds and impure mumonia gas (zornixlgrfrom crude ammoniaca] liquors during thc initial distillation thereof orotherwise ohtained, this completing thc circle of oporation. The sulfateof ammoi'iium thus ohtained is treated as before and the process may berepeated indefinitely and pure ammonia may he produced from crudo liquorby the use of the small amount of sulfate of ammonium originallyemployed and thcl Arotation .of the process may @mtinuc indefinitelywitthput Waste exceptl such as may Aarise by handling of the sulfuricacid and the oxidation' thereof. By careful work this loss isinsignificant compared with the loss of the entire amount of thcsulfuric acid and of all the lime which is unavoidable in the oldprocesses.

In the described process part of the sulfate of ammonium may besubstitut-ed by" other sulfatos, for instance sulfate of potas si`um, orsulfate of sodium, or a mixture of both, in which case, at practicallythe same temperaturesas in the original process; the reactions takeplace in part or altogether according to the following lformulae:

the volatile rai-bon.compounds comprisimgrE alcohol, isoprol'iyl themethyl. alcolici,` eth'y alcohol1 acetone; toluohbenzol, napthalcne andsimilar compounds, all of which arc rcgarded as contributing toexcessive pressures frequently occurring in refrigcrating plants, areeliminated from the amn'ionia andagnmonium sulfate'with the nitroge nousorganic compounds,- Vwhich includes the pyridin CBHSN fand methylaminNHZCH3 groups. This elimination results in pure.

ammonia and pure commercial sulfate of ammonia.

l claim l. In a process of the class specified, distilliug oli theammonia. and volatile ammonium compounds from ammoniacal liquors,combining the same with acid sulfate of ammonium for making neutralsulfate of ammonium and decomposing the neutral sultate of ammonium byheat into free ammonia gas and acid sulfate of ammonium.

Q. In 'a process of theclass specied, distiltingr olf the ammonia andvolatile ammo nium compounds from ammoniaca] liquors, continuingl thesame with acid sulfate ofamr monium for making neutral sulfate ofammonium and decomposing a large part thereof by heat into free ammoniagas and acid sulfate of ammonium.

3. In a process of the class specified, distilling olf ammonia andvolatile ammonium compounds from ammoniacal liquors cornhining the samewith acid sulfate of'a1nmonium for making neutral sulfate of ammoniumdecomposing the neutral sulfate of ammonium or a large portion thereofVby heat into free ammonia. gas adapted for being worked into commercialproducts and acid sulfate of ammonium or pyrosulfate of ainmonium or amixture of both adapted for being returned for use in the beginning ofthe process. Y

4. In a process ofthe class specified, purifying sulfate of ammoniumfrom carbon compounds including nitrogenous-organio compounds by heatingthe unpure salt;V to

such a temperature that the nitrogenous or ,qanic compounds areconverted into ammonium sulfate by reacting with the sulfuric acid ofthe ammonium salt.,

5. In a recess vof the class specified, puri'- fying sul ate of ammoniumfrom carbon compounds including nitrogenous organic compounds comprisingheating the im ure salt under the influence of a blastof airA to suchatemperature that the volatile carbon compounds are volatilized oroxidized and that the nitrogcnous-orgamc compounds vare converted intoammonium sulfate by reacting with the sulfuric acid of the ammoniumvsalt.

fying,r sulfate of ammonium from carbon compounds includingnitrogenous-orfranic compounds, comprising,r heating the impure saltwhile agitating the same, the heatibeing (5. In a process of the classVspecilied, puri-i raised to such a ten-:peinture that the vola,

tile carbon compounds are fvolntili'zcd or oxil A dized and that thenitrogenous-organic com.- pounds are converted into ammonium sulfa'te.

7. In a process of the class specified` distilling ofi' the-:ammonia andvolatile amrn0- nium compounds from amnioniacal' liquors combining thesame with one or more acid ing all or a large part thereof by heat into10 sulfatos to nmke neutral salts and clecomposfree ammonia gas andFyosulfates.

ing ull or u large part thereof by heat into In testimony whereo 'affixmy signature free Ammonia gus und acid sulfatos. in presence of twoWltnesses.

8. In u process of the class s ecfied, distilling ol" the ammonio, ondv0 utile ammo FREDERICK r FRERICHS' nia compounds from ummoniacolliquors, Witnesses: l i' eombimng thelsaxne with one or more acrd M. G.Benjamin, sulfatos to make neutral salts and deeompos E. M. K11-011m.

